CN105712638B - Glass cures polyacrylate super-hydrophilic coating and preparation method thereof with ultraviolet light - Google Patents
Glass cures polyacrylate super-hydrophilic coating and preparation method thereof with ultraviolet light Download PDFInfo
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- CN105712638B CN105712638B CN201510895511.9A CN201510895511A CN105712638B CN 105712638 B CN105712638 B CN 105712638B CN 201510895511 A CN201510895511 A CN 201510895511A CN 105712638 B CN105712638 B CN 105712638B
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Abstract
The invention discloses glass ultraviolet lights to cure polyacrylate super-hydrophilic coating and preparation method thereof.The preparation method is：Hydroxylating is carried out to glass using the concentrated sulfuric acid and hydrogen peroxide first, and it is modified with the silane coupling agent of the double bond containing C=C, the modified glass of surface double bond containing C=C is made；Then at room temperature, hydrophilic acrylate monomer is scattered in absolute ethyl alcohol and stirred evenly, add crosslinking agent and photoinitiator, continued stirring and form uniform solution；Finally, the solution of preparation is coated uniformly on the modified glass of the double bond containing C=C using knife coating, being solidificated in glass surface by ultraviolet light forms one layer of polyacrylate super-hydrophilic coating for having with glass chemical bond linkage.Polyacrylate super-hydrophilic coating prepared by the present invention can effectively avoid hydrophilic coating and the caducous problem of glass surface, and water contact angle is both less than 10 °, have super hydrophilicity, and coating also has good translucency.
Description
Technical field
The present invention relates to a kind of super hydrophilic materials, and in particular to it is super hydrophilic that a kind of glass ultraviolet light cures polyacrylate
Coating and preparation method thereof.
Background technology
Super-hydrophilic coating can make water droplet in the complete drawout in its surface, formation due to its special surface wettability
One layer of very thin moisture film.Normally, coating of the water contact angle up to less than 10 ° is known as super-hydrophilic coating, self-cleaning, anti-
There is very extensive application in the fields such as mist, antifouling, water-oil separating.
At present, there are mainly two types of the approach for preparing super-hydrophilic coating：First, using preparations such as sol-gal process, sedimentations
The inorganic material coatings such as titanium dioxide, zinc oxide, stannic oxide are obtained, then it is irradiated using ultraviolet light, makes surface
Property is changed into Superhydrophilic from hydrophobicity.For example, Yao etc. is first prepared for two using acid catalyzed process and sedimentation in glass surface
The composite coating of silica and titanium dioxide.After ultraviolet light, which has super hydrophilicity and good light transmission
Performance and anti-fog performance, but super hydrophilicity (Yao L, He J H.Facile can be gradually lost after placing it in dark surrounds
dip‐coating approach to fabrication of mechanically robust hybrid thin films
with high transmittance and durable superhydrophilicity.Surface&Coatings
Technology,2014,2(19):6994‐7003)；Second, by being prepared in the surface structure roughness of hydrophilic material
Super-hydrophilic coating.For example, Cebeci etc. sinks polycationic compounds and nano silicon dioxide by the method for LBL self-assembly
It accumulates in glass surface, prepares the super-hydrophilic coating containing porous nanometer structure, and shown good anti-fog performance.
(Cebeci FWu Z H,Zhai L,et al.Nanoporosity‐driven superhydrophilicity:A
means to create multifunctional antifogging coatings.Langmuir,2006,22(6):
2856‐2862).But the super-hydrophilic coating prepared by this method easily comes off under the immersion of wet environment or water,
It is unfavorable for its long-time service, and preparation process is complex, is unfavorable for actual production.
Invention content
The present invention easily influenced for super hydrophilicity existing for current super-hydrophilic coating by light or under the immersion of water it is easy
The defects of coming off provides that a kind of preparation process is simple, performance is stable and can form chemical bond chain with applying interlayer in glass surface
Polyacrylate super-hydrophilic coating connect and preparation method thereof.
The object of the invention is achieved through the following technical solutions：
Glass cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, includes the following steps：
(1) glass is placed in the mixed solution of the concentrated sulfuric acid and hydrogen peroxide, reacts 0.5-1.5h at 80-100 DEG C, take out and use
Deionized water is washed till neutrality；It adds in the ethanol water of silane-containing coupling agent, 0.5- is reacted under the conditions of 60-80 DEG C
1.5h, drying, is then washed with absolute ethyl alcohol, obtains the modified glass of surface double bond containing C=C；The silane coupling agent is γ-first
Three ethoxy of base acryloxypropyl trimethoxy silane (KH-570), vinyltrimethoxysilane (A-171) or vinyl
Base silane (A-151)；
(2) at room temperature, 20-50 parts of hydrophilic acrylate monomers according to the mass fraction, are scattered in 100 parts of anhydrous second
It is stirred evenly in alcohol；2-20 parts of crosslinking agents and 0.5-1.5 parts of photoinitiators are added, is stirred to form homogeneous solution, pass through
Knife coating is coated uniformly on the modified glass of surface double bond containing C=C, under being irradiated under ultraviolet lamp, obtains a kind of glass
Glass cures polyacrylate super-hydrophilic coating with ultraviolet light；The crosslinking agent is pentaerythritol triacrylate, pentaerythrite four
It is one or two kinds of in acrylate, trimethylol-propane trimethacrylate and trimethylolpropane trimethacrylate
Mixture.
Further to realize the object of the invention, it is preferable that the glass is silica containing silicate glass.
Preferably, the hydrophilic acrylate monomer is acryloxyethyldimethyl benzyl ammonium chloride, methyl-prop
Alkene acyloxyethyl dimethyl benzyl ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and acrylyl oxy-ethyl-trimethyl chlorine
Change one or more in ammonium.
Preferably, the photoinitiator is 2- hydroxy-2-methyl -1- phenyl -1- acetone (1173), 1- hydroxy-cyclohexyl benzene
Base ketone (184), 2- methyl-1s-(4- methyl mercaptos phenyl) -2- morpholine -1- acetone (907), 2- benzyl -2- dimethylaminos -1-
One kind in (4- morpholinyl phenyls) butanone (369), phenyl bis- (2,4,6- trimethylbenzoyls) phosphine oxide (819) photoinitiator
Or two kinds of mixture.
Preferably, the mass concentration of the concentrated sulfuric acid is 98%；The mass concentration of the hydrogen peroxide is 30%；The concentrated sulfuric acid and
The mass ratio of hydrogen peroxide is 4:1‐2:1.
Preferably, silane coupling agent accounts for the 3%- of ethanol water quality in the ethanol water of the silane-containing coupling agent
10%；The volume ratio of second alcohol and water is 1:1‐3:1.
Preferably, the drying is placed in placing 0.5-1.5h in 100-120 DEG C of baking oven.
Preferably, the number of the absolute ethyl alcohol washing is 1-3 times.
Preferably, the radiation intensity of the ultraviolet light is 30-100mW/cm2；The time irradiated under the ultraviolet lamp is
60-600 seconds.
A kind of glass cures polyacrylate super-hydrophilic coating with ultraviolet light, is made by above-mentioned preparation method.
Compared with prior art, the invention has the advantages that：
(1) by ultraviolet light curing prepare polyacrylate super-hydrophilic coating, have it is simple for process, production efficiency is high,
The advantages that green non-pollution, and the super hydrophilicity of coating is stablized；
(2) chemical bond linkage is formd between super-hydrophilic coating and glass surface, under the immersion of wet environment or water not
It is easy to fall off；
(3) glass prepared by has good light transmission with polyacrylate super-hydrophilic coating.
Description of the drawings
Fig. 1 is the complete of unmodified glass a, the modified glass b of surface double bond containing C=C and polyacrylate super-hydrophilic coating c
Reflectance infrared spectrum.
Fig. 2 is that the light transmittance that unmodified glass has the glass of polyacrylate super-hydrophilic coating with surface compares.
Specific embodiment
To more fully understand the present invention, with reference to embodiment, the invention will be further described, but the reality of the present invention
It is without being limited thereto to apply mode.
Embodiment 1
It is 3 by the volume ratio that glass is placed in the concentrated sulfuric acid (mass concentration 98%) and hydrogen peroxide (mass concentration 30%):1 it is mixed
It closes in solution, is taken out after reacting 0.75h at 90 DEG C, be washed with deionized to neutrality, place it in the 200g containing KH-570
(KH-570 mass is 10 grams to ethanol water, and the volume ratio of absolute ethyl alcohol and deionized water is 2:1) it in, is reacted at 70 DEG C
1h places 0.5h in 120 DEG C of vacuum drying oven after taking-up, its supersound washing 3 times then is contained C to get surface in ethanol
The modified glass of=C double bonds.
At room temperature, by the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 4g (Jiangsu Feymer Technology Co., Ltd.)
Be added in the absolute ethyl alcohol of 20g, stir evenly, then to its add in 0.75g trimethylolpropane trimethacrylates and 0.2g
Photoinitiator 2- hydroxy-2-methyl -1- phenyl -1- acetone (1173), is stirred to form homogeneous solution, be applied with doctor knife coater
It overlays on the modified glass of surface double bond containing C=C, is 60mW/cm in ultraviolet radiation intensity2Under conditions of cure 120 seconds, make
It obtains a kind of glass and cures polyacrylate super-hydrophilic coating with ultraviolet light, measured water contact angle is listed in table 1.
It will be seen from figure 1 that compared with spectral line a, occur several new absorption peaks on spectral line b：1727cm‐1Locate as C
The stretching vibration absworption peak of ═ O, 1640cm‐1Locate the stretching vibration absworption peak for C ═ C, shake at 983cm-1 for the flexible of Si-OH
Dynamic absorption peak, 1481cm‐1For CH2Deformation vibration peak, 1155cm‐1Locate the asymmetric stretching vibration peak for Si-O-Si, these peaks
Appearance show that KH-570 has been grafted to glass surface；In spectral line c, 1092cm‐1Locate it is corresponding be ammonium absorption peak,
2850cm‐1And 2925cm‐1Locate it is corresponding be C-H stretching vibration absworption peak, 1725cm‐1Locate the stretching vibration peak for C ═ O,
1300cm‐1Locate for C-O stretching vibration peaks, to show MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and trimethylolpropane tris propylene
Acid esters participates in polymerisation and forms coating on modified glass surface.
Figure it is seen that in 400nm hereinafter, there is the light transmittance of the glass of polyacrylate super-hydrophilic coating on surface slightly
Less than unmodified glass；And in more than 400nm, the light transmittance of the two is basically identical.This shows prepared super-hydrophilic coating tool
There is good translucency.
Embodiment 2
It is 4 by the volume ratio that glass is placed in the concentrated sulfuric acid (mass concentration 98%) and hydrogen peroxide (mass concentration 30%):1 it is mixed
It closes in solution, is taken out after reacting 1.5h at 80 DEG C, be washed with deionized to neutrality, place it in the 200g second containing A-171
(A-171 mass is 15 grams to alcohol solution, and the volume ratio of absolute ethyl alcohol and deionized water is 3:1) in, 0.5h is reacted at 80 DEG C,
1h is placed after taking-up in 110 DEG C of vacuum drying oven, it is then in ethanol that its supersound washing 3 times is bis- containing C=C to get surface
The modified glass of key.
At room temperature, the acrylyl oxy-ethyl-trimethyl salmiac of 5g (circle in the air Chemical Group in Jiangsu) is added to 20g's
It in absolute ethyl alcohol, stirs evenly, then 0.4g pentaerythritol tetraacrylates and 0.15g photoinitiators 184 is added in it, stirring is mixed
Conjunction forms homogeneous solution, is coated onto on the modified glass of surface double bond containing C=C with doctor knife coater, in ultraviolet radiation intensity
For 50mW/cm2Under conditions of cure 400 seconds, be made a kind of glass with ultraviolet light cure polyacrylate super-hydrophilic coating, surveyed
The water contact angle obtained is listed in table 1.
Embodiment 3
It is 2 by the volume ratio that glass is placed in the concentrated sulfuric acid (mass concentration 98%) and hydrogen peroxide (mass concentration 30%):1 it is mixed
It closes in solution, is taken out after reacting 0.5h at 100 DEG C, be washed with deionized to neutrality, place it in the 200g second containing A-151
(A-171 mass is 6 grams to alcohol solution, and the volume ratio of absolute ethyl alcohol and deionized water is 2:1) in, 1.5h is reacted at 60 DEG C,
1.5h is placed after taking-up in 100 DEG C of vacuum drying oven, its supersound washing 3 times is then contained into C=C to get surface in ethanol
The modified glass of double bond.
At room temperature, the methylacryloxyethyldimethyl benzyl ammonium chloride of 10g (circle in the air Chemical Group in Jiangsu) is added
Enter into the absolute ethyl alcohol of 20g, stir evenly, then 2g pentaerythritol triacrylates and 0.3g photoinitiators 907 are added in it,
It is stirred to form homogeneous solution, be coated onto on the modified glass of surface double bond containing C=C with doctor knife coater, in ultraviolet light spoke
Intensity is penetrated as 100mW/cm2Under conditions of cure 60 seconds, be made a kind of glass with ultraviolet light cure the super hydrophilic painting of polyacrylate
Layer, measured water contact angle are listed in table 1.
Embodiment 4
It is 5 by the volume ratio that glass is placed in the concentrated sulfuric acid (mass concentration 98%) and hydrogen peroxide (mass concentration 30%):2 it is mixed
It closes in solution, is taken out after reacting 1h at 85 DEG C, be washed with deionized to neutrality, place it in the 200g ethyl alcohol containing KH-570
(KH-570 mass is 20 grams to aqueous solution, and the volume ratio of absolute ethyl alcohol and deionized water is 3:1) in, 0.75h is reacted at 75 DEG C,
1.5h is placed after taking-up in 105 DEG C of vacuum drying oven, its supersound washing 3 times is then contained into C=C to get surface in ethanol
The modified glass of double bond.
At room temperature, it is the acryloxyethyldimethyl benzyl ammonium chloride of 6g (Zibo Wan Duofu Chemical Co., Ltd.s) is molten
Liquid is added in the absolute ethyl alcohol of 20g, is stirred evenly, then adds in 4g trimethylolpropane trimethacrylates and 0.25g light to it
Initiator 369, is stirred to form homogeneous solution, is coated onto on the modified glass of surface double bond containing C=C with doctor knife coater,
It is 40mW/cm in ultraviolet radiation intensity2Under conditions of cure 400 seconds, be made a kind of glass with ultraviolet light cure polyacrylic acid
Ester super-hydrophilic coating, measured water contact angle are listed in table 1.
Embodiment 5
It is 3 by the volume ratio that glass is placed in the concentrated sulfuric acid (mass concentration 98%) and hydrogen peroxide (mass concentration 30%):1 it is mixed
It closes in solution, is taken out after reacting 1h at 95 DEG C, be washed with deionized to neutrality, place it in the 200g ethyl alcohol containing A-151
(A-151 mass is 20 grams to aqueous solution, and the volume ratio of absolute ethyl alcohol and deionized water is 1:1) in, 1.5h is reacted at 65 DEG C, is taken
0.5h is placed after going out in 120 DEG C of vacuum drying oven, it is then in ethanol that its supersound washing 3 times is bis- containing C=C to get surface
The modified glass of key.
At room temperature, 8g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides are added in the absolute ethyl alcohol of 20g, stirring is equal
It is even, then 3g pentaerythritol tetraacrylates and 0.1g photoinitiators 819 are added in it, it is stirred to form homogeneous solution, with scraping
Painting machine is coated onto on the modified glass of surface double bond containing C=C, is 30mW/cm in ultraviolet radiation intensity2Under conditions of it is solid
Change 600 seconds, a kind of glass is made and cures polyacrylate super-hydrophilic coating with ultraviolet light, measured water contact angle is listed in table 1.
1 glass of table cures the water contact angle of polyacrylate super-hydrophilic coating with ultraviolet light
Table 1 cures the water contact angle of polyacrylate super-hydrophilic coating for glass ultraviolet light, is public using Germany KRUSS
What the DSA100 contact angle testers of department were tested.From table 1 it follows that the water contact of glass polyacrylate coatings
Angle is both less thanHave super hydrophilicity, can be applied to windshield and rearview mirror, glass of building window and curtain wall,
The fields such as traffic sign, ad decoration can play antifog and self-cleaning function.
Ultraviolet light curing polyacrylate super-hydrophilic coating prepared by the present invention is using hydrophilic monomer, in ultraviolet light
Irradiation and photoinitiator initiation under, obtain in a short time, therefore have the characteristics that simple for process, production efficiency is high.
Under dark surrounds, the hydrophilicity of the inorganic super-hydrophilic coating such as titanium dioxide can gradually be lost, and the polypropylene in the present invention
The super hydrophilicity of acid esters coating will not be then affected by this, and can keep stable in a long time.Further, since it is grafted on glass
The C=C double bonds of the KH-570 on glass surface can be connected coating and glass in the form of chemical bond by participating in polymerization, this
Sample avoids coating caducous phenomenon under the immersion of wet environment or water.
Claims (9)
1. glass cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, it is characterised in that includes the following steps：
(1) glass is placed in the mixed solution of the concentrated sulfuric acid and hydrogen peroxide, 80-100 DEG C react 0.5-1.5h, taking-up spend from
Son is washed to neutrality；It adds in the ethanol water of silane-containing coupling agent, 0.5-1.5h is reacted under the conditions of 60-80 DEG C, dry
It is dry, it is then washed with absolute ethyl alcohol, obtains the modified glass of surface double bond containing C=C；The silane coupling agent is γ-metering system
Acryloxypropylethoxysilane trimethoxy silane, vinyltrimethoxysilane or vinyltriethoxysilane；The silane-containing coupling
Silane coupling agent accounts for the 3%-10% of ethanol water quality in the ethanol water of agent；The volume ratio of second alcohol and water is 1:1‐3:
1；
(2) at room temperature, according to the mass fraction, 20-50 parts of hydrophilic acrylate monomers are scattered in 100 parts of absolute ethyl alcohols
It stirs evenly；2-20 parts of crosslinking agents and 0.5-1.5 parts of photoinitiators are added, are stirred to form homogeneous solution, pass through blade coating
Method is coated uniformly on the modified glass of surface double bond containing C=C, under being irradiated under ultraviolet lamp, is obtained a kind of glass and is used
Ultraviolet light cures polyacrylate super-hydrophilic coating；The crosslinking agent is pentaerythritol triacrylate, pentaerythrite tetrapropylene
One or two kinds of mixing in acid esters, trimethylol-propane trimethacrylate and trimethylolpropane trimethacrylate
Object.
2. glass according to claim 1 cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, special
Sign is：The glass is silica containing silicate glass.
3. glass according to claim 1 cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, special
Sign is：The hydrophilic acrylate monomer is acryloxyethyldimethyl benzyl ammonium chloride, methacryloxypropyl second
In base dimethyl benzyl ammonium chloride, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride and acrylyl oxy-ethyl-trimethyl salmiac
It is one or more.
4. glass according to claim 1 cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, special
Sign is：The photoinitiator for 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- hydroxycyclohexyl phenyl ketones, 2- methyl -
1- (4- methyl mercaptos phenyl) -2- morpholine -1- acetone, 2- benzyl -2- dimethylaminos -1- (4- morpholinyl phenyls) butanone, phenyl are double
One or two kinds of mixture in (2,4,6- trimethylbenzoyls) phosphine oxide photoinitiator.
5. glass according to claim 1 cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, special
Sign is：The mass concentration of the concentrated sulfuric acid is 98%；The mass concentration of the hydrogen peroxide is 30%；The concentrated sulfuric acid and hydrogen peroxide
Mass ratio is 4:1‐2:1.
6. glass according to claim 1 cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, special
Sign is：The drying is placed in placing 0.5-1.5h in 100-120 DEG C of baking oven.
7. glass according to claim 1 cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, special
Sign is：The number of the absolute ethyl alcohol washing is 1-3 times.
8. glass according to claim 1 cures the preparation method of polyacrylate super-hydrophilic coating with ultraviolet light, special
Sign is：The radiation intensity of the ultraviolet light is 30-100mW/cm2；The time irradiated under the ultraviolet lamp is 60-600 seconds.
9. a kind of glass cures polyacrylate super-hydrophilic coating with ultraviolet light, it is characterised in that it is any by claim 1-8
The item preparation method is made.
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| CN111807711B (en) * | 2020-07-24 | 2022-05-13 | 江苏秀强玻璃工艺股份有限公司 | Manufacturing process of super-hydrophilic long-life organosilicon quaternary ammonium salt antibacterial glass |
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| CN116041998B (en) * | 2022-12-02 | 2024-04-30 | 国家电投集团杭州新能源生产运营有限公司 | Super-hydrophilic coating composition, super-hydrophilic coating and preparation method thereof |
| CN115717005A (en) * | 2022-12-02 | 2023-02-28 | 浙江省白马湖实验室有限公司 | Super-hydrophilic self-cleaning coating composition and preparation method thereof |
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